materials

Article
Ultra High Strain Rate Nanoindentation Testing
Pardhasaradhi Sudharshan Phani 1, * and Warren Carl Oliver 2
1 International Advanced Research Centre for Powder Metallurgy and New Materials (ARCI), Balapur PO,
Hyderabad, Telangana 500005, India
2 Nanomechanics Inc., 105 Meco Ln, Oak Ridge, TN 37830, USA; [email protected]
* Correspondence: [email protected]; Tel.: +91-40-2445-2418; Fax: +91-40-2444-3168

Received: 20 May 2017; Accepted: 14 June 2017; Published: 17 June 2017

Abstract: Strain rate dependence of indentation hardness has been widely used to study
time-dependent plasticity. However, the currently available techniques limit the range of strain
rates that can be achieved during indentation testing. Recent advances in electronics have enabled
nanomechanical measurements with very low noise levels (sub nanometer) at fast time constants
(20 µs) and high data acquisition rates (100 KHz). These capabilities open the doors for a wide range
of ultra-fast nanomechanical testing, for instance, indentation testing at very high strain rates. With an
accurate dynamic model and an instrument with fast time constants, step load tests can be performed
which enable access to indentation strain rates approaching ballistic levels (i.e., 4000 1/s). A novel
indentation based testing technique involving a combination of step load and constant load and hold
tests that enables measurement of strain rate dependence of hardness spanning over seven orders of
magnitude in strain rate is presented. A simple analysis is used to calculate the equivalent uniaxial
response from indentation data and compared to the conventional uniaxial data for commercial
purity aluminum. Excellent agreement is found between the indentation and uniaxial data over
several orders of magnitude of strain rate.

Keywords: high strain rate; nanoindentation; aluminum alloy; dynamics

1. Introduction
Measuring the strain rate dependence of flow stress is of great interest to the materials community
and has been a widely-studied research area [1]. The strain rate dependence of flow stress of bulk
materials can be routinely measured over a wide range using many conventional techniques like
uniaxial compression/tension for lower strain rates and Split-Hopkinson pressure bar for high strain
rates [2]. However, these techniques are not readily applicable for small-scale structures or small
volumes of materials, which has been a recent area of focus for the materials community. Several
groups have used micro/nano impact testing [3–5] or dynamic indentation to understand the high
strain rate behavior without necessarily using the depth sensing capability and they mostly fall under
the microindentation regime [6–11]. Techniques based on nanoindentation such as constant strain
rate test, strain rate jump test, constant rate of loading test, or a constant load and hold test have
been widely used to measure the rate dependence of hardness of small volumes of materials over a
range of strain rates [12–16]. These techniques are typically limited to the lower strain rate regimes
(<1 1/s). In order to access high strain rates during indentation, a step load test can be performed,
wherein, the load is ramped within a few micro seconds [14]. This results in sweeping across a wide
range of strain rates especially in the high strain rate regime (>100 1/s) in a single test. This could be a
powerful technique to measure the high strain rate response at small scales in a simple, quick, and
cost-effective way.
While the step load test theoretically offers a great opportunity to probe the material response
at high strain rates, there are several experimental challenges, such as the dynamic contribution

Materials 2017, 10, 663; doi:10.3390/ma10060663 www.mdpi.com/journal/materials

Materials 2017, 10, 663 2 of 12

of the instrument and the time constants of the measurement signals, which need to be carefully
considered in order to make valid measurements. Recent advances in electronics have enabled
nanomechanical measurements with very low noise levels (sub nanometer) at fast time constants
(20 µs) and high data acquisition rates (100 KHz). These capabilities open the doors for a wide
range of ultra-fast nanomechanical testing. In addition to having a measuring instrument with fast
response, a comprehensive model for the dynamics of the instrument and measurement electronics is
required to make accurate high strain rate measurements. In this work, we present a step load-based
indentation high strain rate measurement technique that relies on fast response instrumentation and
a comprehensive model for the instrument’s dynamics and electronics. High strain rate tests are
performed on annealed commercial purity aluminum alloy (1100 Al) to demonstrate the technique. A
simple analysis is used to calculate the uniaxial equivalent response from the indentation results and is
compared to the conventional high strain rate tests to assess the accuracy of this technique. The relative
contribution of the instrument’s dynamic response and the time constants of the measurement signals
to the overall measurement are also discussed to demonstrate the importance of accurate instrument
characterization for high strain rate indentation testing.

2. Experimental Procedure and Calculations

2.1. Measuring Strain Rate Dependence of Hardness

As mentioned earlier, indentation based techniques have been widely used to measure the strain
rate dependence of hardness in the lower strain rate regime (<1 1/s). The strain rate during an
indentation test is often defined as the ratio of the indenter velocity to the depth of indentation.
Accessing higher strain rates requires higher indentation velocities at a given depth, or a lower depth
for a given velocity or a combination of both. In order to minimize the contributions from indentation
size effect (ISE) [17], it is preferable to access higher strain rates by achieving higher velocities at large
depths. This can be accomplished by performing a step load test wherein the force is ramped as fast as
the actuator used can physically accomplish the change. This results in sweeping a wide range of strain
rates in the high strain rate regime in a single indentation test. The major requirements to perform
these tests is a testing system with fast response actuators and sensors and a model for instrument’s
dynamics and electronics to accurately factor out the instrument’s contribution from the measured
response. These will be described in greater detail in the subsequent subsections.
Step load tests and the conventional constant load and hold (CLH) indentation tests were
performed to a static load of 16 mN to cover a wide range of indentation strain rates. In both the cases,
the tip is brought in contact with the sample at a slow approach rate of 200 nm/s. The CLH tests were
performed by ramping the load to 16 mN at a loading rate of 5 N/s after contact and subsequently
maintaining a constant force for 30 s. In the case of step load tests, a step force of 16 mN was input to
the force actuator after contact. Note that the step load tests are not impact tests as the tip approaches
the sample slowly before contact and the fast loading is only after contact. Unlike the CLH test, due to
the fast loading in a step load test, there are significant inertial effects which result in actual load on
sample being much higher than the applied step force of 16 mN for a short span. This is immediately
followed by a decrease in the load on the sample due to the exhaustion of the dynamic forces, resulting
in unloading of the contact even while the actuator applies the 16 mN force. This will be discussed
in greater detail in Section 3.1. All the tests were performed on a 10 mm diameter commercial purity
aluminum (1100 aluminum) sample which was polished and subsequently annealed at 350 ◦ C for 4 h
before testing. Ten repetitive step load and CLH tests were performed to ensure repeatability in the
data. A diamond Berkovich tip (Micro Star Technologies, Huntsville, TX, USA) was used for all the
tests. The load frame stiffness determination and tip area calibration was done using the results of
constant strain rate tests (0.2 1/s) on fused silica. For these tests, the contact stiffness was continuously
measured as a function of depth using a phase lock amplifier (Nanomechanics Inc., Oak Ridge, TN,
USA) oscillating at 100 Hz frequency and a 2 nm displacement amplitude.
Materials 2017, 10, 663 3 of 12

2.2. Measuring Instrumentation

In order to perform a step load test, the testing system requires a force actuator that can apply the
desired force in a short time interval, which is typically less than a millisecond, and a displacement
sensor that can accurately capture the rapid change in the displacement during that time. In addition, a
high data acquisition rate is required. In a typical commercially-available nanoindentation system with
an electromagnetic actuator, force is controlled by the current to the coil, which is a command signal,
and the displacement is measured by a capacitance gage, which is a measured signal. To perform a
step load test, a step function in current is sent as a command input to the actuator. Due to the finite
time constant of the force signal, the actual force delivered by the actuator is not an instantaneous
step function, but an exponential function with a finite rise time. The time constant of a signal is a
parameter that characterizes the response of a signal to a unit step input. For first order linear-time
invariant systems, it is the time required to reach 63% of its step input value or one third the time
required to reach 95% of its step input. Hence, if the time scale of the test is comparable to the time
constants of the measurement signals, corrections to the signals are required. In order to minimize
these corrections, it is desirable to have measurement time constants much shorter than the time scale
of measurement.
The step load tests in the current work were performed using a commercially available
nanoindenter, iNano® from Nanomechanics Inc., Oak Ridge, TN, USA. It uses an electromagnetically-
actuated InForce50 actuator with a force time constant of 290 µs, a displacement time constant of
20 µs, and data acquisition rate of 100 kHz. Force is the command signal and the displacement is the
measured signal. The displacement sensor has sub nanometer noise levels even at a short time constant
of 20 µs. This is critical for high strain rate testing as the velocity and acceleration are calculated by
taking the first and second derivative of the displacement signal and any noise is amplified, especially
by the second derivative.

2.3. Model for the Instrument’s Dynamics and Electronics

At high strain rates, the instrument’s dynamic contribution can dominate the measured response
and can lead to inaccuracies in the measurement. In order to account for the instrument’s dynamic
contribution, a simple one degree of freedom (one DOF) damped harmonic oscillator model is proposed
to model the electromagnetically-actuated indentation system. A schematic of the model is shown in
Figure 1. The actuator is modeled as a single mass, spring, and dashpot system where the mass, m, is
the moving mass of the coil and the indenter shaft, damping coefficient, b, is the damping generated
due to resistance to the motion of the air in the capacitance gage and the eddy current damping in
an electromagnetic actuator and the spring constant, k, is the spring constant of the leaf springs that
support the indenter shaft. The sample or the contact is modeled as a spring and dashpot, which
represents the contact stiffness and damping, respectively. As the moving mass of the sample is very
small compared to the mass of the system, it is neglected. The load frame which holds the indentation
system is modeled as a spring for simplicity.
The one DOF model shown in Figure 1 is one of the simplest possible dynamic models for an
indentation system and given the complexity of most indentation systems, demonstrating that the
testing system can be accurately described by this model is critical for high strain rate testing where
the instruments contribution can dominate the measured response. Once the simple model for the
actuator is validated its dynamic contribution can be simply factored out to accurately determine the
response of the sample.
In order to validate the one DOF model for the actuator, a frequency sweep experiment is
performed, wherein the actuator is excited dynamically at a fixed sinusoidal force oscillation amplitude
over a wide range of frequency in free air (i.e., without a sample), The resultant dynamic displacement
amplitude and the phase lag between the force and displacement signals are measured using a phase
lock amplifier (PLA). Figure 2a shows the results of a typical frequency sweep experiment for an
InForce50 actuator, wherein the measured dynamic compliance of the instrument in free air, which is
Materials 2017, 10, 663 4 of 12

the ratio of the2017,

Materials dynamic
10, 663 displacement amplitude (h o ) to the dynamic force amplitude (Fo ), is plotted
4 of 12 as
a function of the excitation frequency (ω). This is commonly referred to as the transfer function of the
as the transfer
instrument. The dynamicfunction of the instrument.
compliance (C) andThe dynamic
phase compliance
(ø) for (C) oscillator
a one DOF and phase can
(ø) for
beatheoretically
one DOF
oscillator can be theoretically
calculated using the following equations. calculated using the following equations.

q
C = ho /Fo = ((k − mω 2 )2 + (bω )2 ) (1)
Materials 2017, 10, 663 bω 4 of 12
φ = tan−1 ( 2
) (2)
k − mω
as the transfer function of the instrument. The dynamic compliance (C) and phase (ø) for a one DOF
oscillator can be theoretically calculated using the following equations.

Figure 1. Schematic of the one DOF model for the indentation system showing the various dynamic
elements used for the actuator, sample/contact, and the load frame.

Figure 1. Schematic of the one DOF model for the indentation system showing the various dynamic
elementsof
Figure 1. Schematic used
theforone DOF=
the actuator, ℎ / for = the
sample/contact,
model ((indentation
and the−load frame.
) +system (1)
( ) )showing the various dynamic
elements used for the actuator, sample/contact, and the load frame.
=ℎ / = = tan
(( −( ) + ( ))) ) (1) (2)
−
= tan ( )) (2)
The experimental
The experimental datadatashown shown in the
in the plotplot
cancanbe−befitfittotoaa functional
functional form formgiven given ininEquation
Equation (1) to
(1) to
assess the suitability
The of
experimental using
data the
shown one in DOF
the plotmodel
can be for
fit to athe instrument.
functional
assess the suitability of using the one DOF model for the instrument. The solid red line in the form The
given in solid
Equation red
(1) line
to in the plotplot
assess
onethe suitability of using the the
one DOF model for thedata.
instrument.
This The solid red linedemonstrates
in the plot
shows shows
the onetheDOF
shows the
DOF
model model
fit to
one DOF
fit experimental
the
model
to experimental
fit to the experimentaldata. This
data. Thisplot
plot
plot clearly
clearly
demonstrates
clearly demonstrates
that the
that thethat the actuator
can be actuator can
accurately be accurately
modeled
actuator as amodeled
can be accurately simple
modeledone
asasaa simple
DOFone
simple
one DOF oscillator.
oscillator.
DOF oscillator. TheThemass The mass
(m),
mass (m),
(m),coefficient
damping
damping
damping coefficient
coefficient (b), and
(b), and spring
(b), and constant (k) of
spring constant (k) the
of theactuator usedforfor
actuator used thethe current
current work
work are are
180.45 mg,180.45 mg, 0.106
0.106 Ns/m, and Ns/m, and
spring constant243 (k)N/m,
of respectively.
the actuator used for the current work are 180.45 mg, 0.106 Ns/m, and 243 N/m,
243 N/m, respectively. Figure 2b2b
Figure shows
shows the experimental
the experimental data data and
and the modeltheprediction
model prediction
for the phase for the phase
respectively. Figure
angle between
2b shows
angle between the experimental
the displacement
the displacement andand force signals,
force signals,
data and the
reinforcing
reinforcing
theexcellent
model prediction
agreement
the excellent
for the
in the results
agreement
phase angle
in the results
between observed
the displacement from the transfer function
and force signals, plot and also demonstrating the accuracy of the phase angle
observed from the transfer
measurements. While thefunction
one DOF model plotreinforcing
and alsohere
presented
the excellent the
demonstrating agreement
is simple, it can even be accuracy
used under
inofthe
theresults
non- phase observed
angle
from the transfer
measurements. function
ambient While
conditionsplot and
the(vacuum
one DOF also demonstrating
modeltemperature)
or elevated presentedforherethe accuracy of the
is simple,actuators
electromagnetic phase
it can evenas theybeangle
not measurements.
doused under non-
While the
ambient requiremodel
one DOF a medium
conditions for damping.
presented
(vacuum This enables
here
or elevated high strain
is simple, it can
temperature) ratefor
experiments
even be usedunderunder
electromagnetic vacuum or elevated
non-ambient
actuators as theyconditions
do not
temperatures.
(vacuumrequire a medium
or elevated for damping.for
temperature) This enables high strain
electromagnetic rate experiments
actuators as they do under
not vacuum
require or elevated for
a medium
temperatures.
damping. This enables high strain rate experiments under vacuum or elevated temperatures.

(a) (b)
Figure 2. Comparison of experimental data and one DOF model data for (a) dynamic compliance, and
(b) phase angle of the actuator, as a function of radial frequency for a typical InForce50 actuator.

(a) (b)
Figure 2. Comparison of experimental data and one DOF model data for (a) dynamic compliance, and
Figure 2. Comparison of experimental data and one DOF model data for (a) dynamic compliance, and
(b) phase angle of the actuator, as a function of radial frequency for a typical InForce50 actuator.
(b) phase angle of the actuator, as a function of radial frequency for a typical InForce50 actuator.
Materials 2017, 10, 663 5 of 12

In addition to the dynamic effects of the instrument, understanding and accounting for the time
constants of the measurement signals is important for making accurate high strain rate measurements.
As discussed in Section 2.2, time constant correction to the signals is required if the time scale of testing
is comparable to the measurement time constant. A simple first order correction can be performed to
Materials 2017, 10, 663 5 of 12
the signal to account for the finite time constant, by the following equation:
In addition to the dynamic effects of the instrument, understanding and accounting for the time
˙


ycorris =
constants of the measurement signals ymsd +forymaking
important msd /2τ accurate high strain rate measurements. (3)
As discussed in Section 2.2, time constant correction to the signals is required if the time scale of
.
where ycorr testing
is theiscorrected
comparablesignal,
to the measurement
ymsd is thetime constant. signal,
measured A simpley first is
msd
order
thecorrection can be
rate of change of the
performed to the signal to account for the finite time constant, by the following equation:
measured signal, and τ is the time constant.
̇
While the transfer function plot demonstrates = +that
( )/2
the instrument can be modeled (3) as a one
DOF oscillator,
whereit doesis not prove the
the corrected accuracy
signal, is of
thethe modelsignal,
measured parameters ̇ is the m,rate
b, and k when
of change applied in
of the
conjunctionmeasured
with thesignal,
time andconstantsis the of
time constant.
the force and displacement signals which can have a significant
While the transfer function plot demonstrates that the instrument can be modeled as a one DOF
effect during fast testing. In order to verify the accuracy of the time constant correction and dynamic
oscillator, it does not prove the accuracy of the model parameters m, b, and k when applied in
model, a step load
conjunctiontest
withis the
performed
time constantsin free
of theair wherein
force the forcesignals
and displacement commandwhich cansignal
have aissignificant
instantaneously
stepped to effect
1 mNduringand fast
thetesting.
resultant displacement response is recorded at 100 kHz.
In order to verify the accuracy of the time constant correction and dynamic Figure 3 shows
model, a step load test is performed in free air wherein the force command
the comparison of the experimental data for a typical InForce50 actuator and model prediction for a signal is instantaneously
stepped to 1 mN and the resultant displacement response is recorded at 100 kHz. Figure 3 shows the
one DOF model at different time constants. There is excellent agreement between the experimental
comparison of the experimental data for a typical InForce50 actuator and model prediction for a one
data and model predictions
DOF model at different for
timea 20 µs time
constants. constant
There displacement
is excellent agreement between signal. This demonstrates
the experimental data the
validity of the
andmodel for the instrument’s
model predictions for a 20 µs time dynamics, as well assignal.
constant displacement the electronics and, hence,
This demonstrates can be used
the validity
to accuratelyof the model
factor out forthe
the contribution
instrument’s dynamics, as well as the to
of the instrument electronics
the total and, hence, can be used
measurement whichto will be
accurately factor out the contribution of the instrument to the total measurement which will be
discussed in greater detail in Section 2.4. The plot also shows the predicted response for 1 ms and
discussed in greater detail in Section 2.4. The plot also shows the predicted response for 1 ms and 200
200 ms timems constant displacement
time constant displacement signals
signalswhich showsignificant
which show significant deviation
deviation from thefrom theresponse.
actual actual response.
Note that the data
Note thatacquisition rate forrate
the data acquisition allfor
of all
theofcurves is 100
the curves kHz
is 100 kHzandand the difference
the difference is is
onlyonly in the time
in the
time constant.
constant. While havingWhile a high having
dataa high data acquisition
acquisition rate israte is important,
important, thisplot
this plot clearly
clearly demonstrates
demonstrates the
the need for a short time constant to accurately capture dynamic events.
need for a short time constant to accurately capture dynamic events.

Figure 3. Comparison of experimental data and model predictions at different displacement time
Figure 3. Comparison of the
constants (tc.) for experimental dataofand
step load response modelinpredictions
the actuator at different
free air for a typical InForce50displacement
actuator. time
constants (tc.) for the step load response of the actuator in free air for a typical InForce50 actuator.
2.4. Calculation of the Indentation Strain Rate and Hardness

2.4. Calculation This

of the Indentation
section presents Strain Rate and
the procedure Hardnessthe indentation strain rate and hardness from
for calculating
the basic measurements, viz., force and displacement. As mentioned earlier, indentation strain rate
This section presents
is the ratio the procedure
of indenter velocity (ℎ̇ )for
to calculating the indentation
the depth of penetration (h). Thestrain
depth rate and hardness
of penetration is from
calculated by subtracting the displacement of the surface point from the measured displacement.
the basic measurements, viz., force and displacement. As mentioned earlier, indentation strain rate is The
.
velocity (ℎ̇) and acceleration (ℎ̈) are calculated by taking the analytical first and second derivative,
the ratio of indenter velocity (h) to the depth of penetration (h). The depth of penetration is calculated
respectively, of the spline fit to the displacement-time response. In order to calculate the load on the .
by subtracting the displacement of the surface point from the measured displacement. The velocity (h)
..
and acceleration (h) are calculated by taking the analytical first and second derivative, respectively,
of the spline fit to the displacement-time response. In order to calculate the load on the sample, the
Materials 2017, 10, 663 6 of 12

dynamic contribution of the instrument needs to be factored out. This can be done by using the simple
one DOF model for the actuator which has been shown to accurately describe the system in Section 2.3.
The equation to calculate the load on the sample (P) factoring out the dynamic contribution of the
instrument, is as follows: . ..
P = F − kh − bh − m h (4)

where F is the force output of the actuator and h is the depth of penetration into the surface. Note
that the load on the sample can be very different from the force output of the actuator depending
on the dynamic contributions of the instrument. This difference is quite significant for the step load
..
tests where the inertial term (mh). dominates. For the case of the constant load and hold tests the
contribution from the damping (b h) and inertial terms is negligible as expected for static indentation.
Once the load on sample is calculated from Equation (4), the hardness is calculated using the
conventional formula of load over the contact area. The contact area is calculated from the tip area
function assuming a constant ratio of contact depth to total depth which, for this case, is found to be
0.99 based on the unloading data of the CLH tests.

2.5. Estimating Equivalent Uniaxial Response

The experimental procedure and calculations described in the earlier sections enable the
determination of hardness as a function of the indentation strain rate. However, in order to compare
the data to the conventional measurements, which are based on uniaxial testing, uniaxial equivalent
parameters have to be estimated from the indentation data, which is challenging given the complexity
of the stress fields during indentation. Recently, Su et al. [18] proposed a simple experimental technique
based on the theoretical analysis of Bower et al. [19] to determine uniaxial creep parameters from
indentation. The equations used to calculate the uniaxial equivalent strain rate and stress are presented
.
here while the details can be found in Su et al. [18]. The equivalent uniaxial strain rate (ε) and stress (σ )
for a power-law creeping solid can be calculated from the basic indentation measurements (h and P)
using the following equations:    
. 1 1 dh
ε= (5)
c tan θ h dt
 " #
1 P
σ= (6)
Fc2 π (h tan θ )2
In the above equations, θ is the equivalent half cone angle, which is 70.3◦ for a Berkovich indenter
and F and c are akin to constraint factor and pile-up/sink-in parameter, respectively. F and c are a
function of the stress exponent and cone angle, and their functional dependence can be obtained from
the recent work of Su et al. [18].

3. Results and Discussion

3.1. Step Load and Constant Load and Hold Tests: Basic Measurements
The depth of penetration into the sample as a function of the time on the sample in response to a
16 mN step force input is shown in Figure 4. Data from 10 tests recorded at 100 kHz is shown in the
plot. Excellent repeatability can be observed from the plot. The depth increases to a maximum value
and subsequently oscillates, wherein the contact is being unloaded and reloaded without causing
further penetration. Hence, the depth up to the point of first maximum represents the elastoplastic
regime which is of interest in the current analysis. The maximum depth is reached in less than 500 µs,
after which the contact oscillates and hence having fast response and low noise displacement sensors
is very important to perform these tests. The load on the sample during this time can be calculated
by factoring out the dynamic contribution of the instrument from the force generated by the actuator
using Equation (4).
Materials 2017, 10, 663 7 of 12
Materials 2017, 10, 663 7 of 12

Materials 2017, 10, 663 7 of 12

Figure 4. Indentation depth as a function of the time on the sample during the step force input of 16
Indentation
Figure 4.mN depth
for 10 different testsas a function
shown of the
in different time on the sample during the step force input of
colors.
16 mN for 10 different tests shown in different colors.
Figure 5 shows the load on sample calculated using Equation (4) for the step load tests. Good
repeatability can be observed even in this case, in spite of having to use the first and second
Figure 5 shows the load on sample calculated using Equation (4) for the step load tests. Good
derivatives of the displacement signal for load calculations. Similar to the depth-time response shown
repeatability can be
in Figure observed
4, the load on sampleeven inreachesthis case, in spitevalue
a maximum of having
whichto use
is at thethepeakfirst andThe
depth. secondmaximum derivatives
of the displacement
load on sample signal for load
(~25 mN) is muchcalculations.
higher thanSimilarthe forcetooutputthe depth-time
of the actuator response
(16 mN)shown which isindue Figure 4,
the load toondynamic
sample reachesfrom
Figure 4.overload
Indentation a maximum
depth as a functionvalue
deceleration of which
thetime
of the tip.onDuetheisto at
samplethethe peak
dynamic
during depth.
nature
the step forceof The maximum
thisoftest
input 16 and the load
on sample experimental
mN for
(~25 mN)10challenges
different
is much described
tests earlier,
shown in different
higher than analyzing
colors.
the force outputthe results of these
of the tests is(16
actuator quitemN) challenging.
which is due
There are contributions from ISE, the inertia of the instrument, the time constant of the command and
to dynamic overload
Figure 5 shows
from deceleration ofcalculated
the tip. usingDueEquation
to the dynamic nature of this test and the
measurement signals,the and loadtheon sample
data acquisition rate which need to (4) for the step
be carefully load tests. During
considered. Good the
experimental
initial
challenges
repeatability
part of can
described
be observed
the step load (<100
earlier,
even analyzing
µs),in calculating
this case, in the
thespite
results
of havingwhich
acceleration,
of these
to useis the tests
the first
second
is quite
andderivative
second challenging.
of
There aredisplacement
contributions
derivatives of the from as ISE,
displacement
is difficult there theareinertia
signalonly 10of
for load thepoints
instrument,
calculations.
data Similar
(data points the
toaretime
the 10 µsconstant
depth-time of the
response
apart in time). command
shown
Even though and
measurement in Figure 4, the and load on thesample reaches a maximumwhich value which isto at the peak depth.considered.
The maximumDuring the
there issignals,
good repeatability data
in theacquisition
results, datarate at such shortneed be carefully
time intervals may not be accurate. As we
load on sample (~25 mN) is much higher than the force output of the actuator (16 mN) which is due
proceed
initial part of thefurther
step in time(<100
load up to 250 µs),µs,calculating
the strain rates the areacceleration,
very high (>10 which 4 1/s) as shown
is the in Figure 6,
second which
derivative of
to dynamic overload from deceleration of the tip. Due to the dynamic nature of this test and the
is
displacement beyond the scope
is difficult of the
as there simple analysis
are only presented
10analyzing
data pointsin the current work,
(dataofpoints where a power
areis10quite µs apart law behavior is
in time). Even
experimental challenges described earlier, the results these tests challenging.
assumed for the strain rate dependence of the flow stress. There may be other physical phenomena that
though thereThere isare
good repeatability
contributions from ISE, in the
theinertia
results, data
of the at suchthe
instrument, short
time time
constantintervals
of the command may not andbe accurate.
are operative atsignals,
measurement such high andstrain
the rates
data which arerate
acquisition notwhich
modeled need here.
to beIncarefully
addition,considered.
the ISE is found 4During to the
exhaust
As we proceed
after further
a depth in time up to 250 µs, the strain rates are very high (>10 it is not as
1/s) shown in
initial part ofofthe1.2step
µm,load which corresponds
(<100 to a time
µs), calculating the on sample ofwhich
acceleration, 340 µs.isFurthermore,
the second derivative ideal
of to
Figure 6,use which
displacement
is than
data less beyond the time
is difficult
the scope
constant
as there
ofthe
of
are only
the
10load
simple
datasignal
analysis
points which is 290presented
(data points µs.10
are Inµsview
apart
ininthe
of the current
constraints
time). Even though
work, where
discussed
a power above,
law behaviorload is
data assumed
beyond 340 for
µs, the
up tostrain
the rate
point of dependence
reaching the maximumof the
there is good repeatability in the results, data at such short time intervals may not be accurate. As we for
step flow
depth stress.
(440 µs) is There
useful may be
the current
proceed analysis.
further in It
time may
up to be noted
250 µs, that
the the
strain contact
rates are unloads
other physical phenomena that are operative at such high strain rates which are not modeled here.
very high completely
(>10 4 1/s) as at ~500
shown µs
in and
Figure the6, load
which on the
sample
In addition, thecalculation
is beyond ISEtheisscope
found based toon
of the Equation
simple
exhaust (4)presented
analysis
after isanot valid
depth beyond
inofthe1.2 thatwork,
current
µm, point.
which where a power law to
corresponds behavior
a timeis on sample
assumed for the strain rate dependence of the flow stress. There may be other physical phenomena that
of 340 µs. are
Furthermore, it is not ideal to use data less than the time constant of the load signal which
operative at such high strain rates which are not modeled here. In addition, the ISE is found to exhaust
is 290 µs. after
In view ofofthe
a depth constraints
1.2 µm, discussed
which corresponds above,
to a time step load
on sample of 340 data beyond 340
µs. Furthermore, it is not up to
µs,ideal to the point
of reachingusethe
datamaximum depth
less than the time (440ofµs)
constant is useful
the load for the
signal which current
is 290 analysis.
µs. In view It maydiscussed
of the constraints be noted that the
above, step
contact unloads load data beyond
completely 340 µs
at ~500 µs, up
andto the
thepoint
loadofon
reaching the maximum
the sample depth (440
calculation µs) is useful
based for
on Equation (4) is
the current analysis. It may be noted that the contact unloads completely at ~500 µs and the load on the
not valid beyond that point.
sample calculation based on Equation (4) is not valid beyond that point.

Figure 5. The load on the sample as a function of time on the sample calculated by accounting for the
dynamic contribution of the instrument during the step load for 10 different tests shown in different
colors.

Figure 5. The load on the sample as a function of time on the sample calculated by accounting for the
The load
Figure 5. dynamic on the ofsample
contribution as a function
the instrument during the of
steptime on10the
load for sample
different testscalculated by accounting
shown in different
for the dynamic
colors. contribution of the instrument during the step load for 10 different tests shown in
different colors.
Materials 2017,10,
Materials2017, 10,663
663 8 8ofof1212
Materials 2017, 10, 663 8 of 12

Figure 6. Indentation
Figure strain
6. Indentation rate
strain rateasasa afunction
functionofoftime
time during
during the
the step force input
step force inputofof16
16mN
mNfor
for1010
Figure 6. Indentation strain rate as a function of time during the step force input of 16 mN for
different tests
different shown
tests in in
shown different colors.
different colors.
10 different tests shown in different colors.

Figure
Figure 7 shows
7 shows thethe indentationdepth
indentation depthasasaafunction
functionof oftime
time on sample
sample for forthe
theCLH
CLHtests.
tests.The
Theplot
plot
Figure
shows
shows 7distinct
twotwo shows theregions:
distinct indentation
regions: thefast
the depth
fast initialas
initial a function
increase
increase of time
indepth
in depth on sample for
corresponding
corresponding to thefast
tothe
the CLH
fast tests.
load
load ramp
rampThe
(5(5
plot shows
N/s) andtwo
the distinct regions:
subsequent creep the
at fast
a initial
fixed forceincrease
of 16 mN.in depth
The corresponding
creep rate in the to
hold
N/s) and the subsequent creep at a fixed force of 16 mN. The creep rate in the hold segment is almost the fast
segment load
is ramp
almost
(5insignificant
N/s) and the as subsequent
insignificant as expected
expected creep
forfor at a fixed
aluminum
aluminum force
atatroom
room of 16 mN. The
temperature
temperature creep
and the
and the data
datarate
mayinnot
may thecorrespond
not hold segment
correspond is
totothe
the
almoststeady
steady state creep
insignificant
state creep asas
as discussed
expected
discussed ininthe
for theprevious
previous
aluminum workof
atwork
room ofthe
the authors
authorsand
temperature [20].
the data may not correspond
[20].
to the steady state creep as discussed in the previous work of the authors [20].

Figure
Figure 7. Indentation
7. Indentation depth
depth as aasfunction
a function of time
of time during
during theCLH
the CLHtest
testfor
for10
10different
different tests
tests shown
shown in
in
different
different
Figure 7. colors.
colors.
Indentation depth as a function of time during the CLH test for 10 different tests shown in
different colors.
3.2. Strain Rate Effects
3.2. Strain Rate Effects
3.2. StrainIn Rate Effects we present the strain rate dependence of hardness for the step load tests and the
this section,
In this section, we present the strain rate dependence of hardness for the step load tests and the
CLH tests. Figure 8 shows the hardness as a function of indentation strain rate for the step load tests.
In this
CLH tests. section,
Figure we present
8 shows the strain
the hardness as rate dependence
a function of hardness
of indentation forrate
strain the for
steptheload
steptests
loadand the
tests.
The hardness and the indentation strain rate are calculated using the procedure described in Section
CLH
The tests. Figure
hardness and the8 shows the hardness
indentation strain rateas are
a function of indentation
calculated strain rate
using the procedure for the step
described load tests.
in Section 2.4.
2.4. The plot also shows the time on sample at the extremes of the data. As discussed in Section 3.1,
Theplot
The hardness and the indentation strain rate
the are calculatedtheusing the
Asprocedure described
Section in Section
data also shows
between 340the time440
µs and on µs
sample
data isatrelevant
extremes
for theof
current data. discussed
analysis. Within thisinwindow, 3.1, data
the step
2.4.load
betweenThe 340
plot also shows the time on sample at the extremes of the data. As discussed in
tests enable access to very high strain rates (4000 1/s). In addition, a range of strain rates atstep
µs and 440 µs data is relevant for the current analysis. Within this window, Section
the 3.1,
the
datahigher
load between
tests enable 340 µs
accessandto 440
veryµs data
high is relevant
strain rates for the
(4000 current
1/s). In analysis.
addition, Within
a range this
of
end can be accessed in a single test which is simple and quick to perform compared to most window,
strain ratesthe
at step
the
loadconventional
higher tests
end enable access
can behigh
accessed to very
strain in high strain
a single
rate tests. rates is
test which (4000 1/s).and
simple In addition, a range of
quick to perform strain rates
compared at the
to most
higher end can
conventional highbestrain
accessed
rate in a single test which is simple and quick to perform compared to most
tests.
conventional high strain rate tests.
Materials
Materials2017, 10,10,
2017, 663663 9 of 12 12
9 of
Materials 2017, 10, 663 9 of 12

Figure 8. Indentation hardness as a function of indentation strain rate for step load tests.
Figure
Figure 8. 8. Indentation
Indentation hardness
hardness asas a function
a function of of indentation
indentation strain
strain rate
rate forfor step
step load
load tests.
tests.
Unlike the step load tests, the variation in hardness as a function of indentation strain rate for
Unlike the step load tests, the variation in hardness as a function of indentation strain rate for
theUnlike
CLH tests the is calculated
step load tests,fromthethe data in in
variation thehardness
hold segment. The calculation
as a function procedure
of indentation strainis similar
rate forto
the CLH tests is calculated from the data in the hold segment. The calculation procedure is similar to
the
the CLHcasetests
of step load, but from
is calculated the load
the on
datathe
insample
the hold does not have
segment. Theany significant
calculation dynamiciscontribution
procedure similar to
the case of step load, but the load on the sample does not have any significant dynamic contribution
from
the casethe of instrument.
step load, but Figure 9 shows
the load thesample
on the hardness
does asnot
a function
have any of significant
indentationdynamic
strain rate for the CLH
contribution
from the instrument. Figure 9 shows the hardness as a function of indentation strain rate for the CLH
tests.
from theThe data fromFigure
instrument. the step load tests
9 shows are also shown
the hardness for comparison.
as a function The strain
of indentation data from the the
rate for CLH CLHtests
tests. The data from the step load tests are also shown for comparison. The data from the CLH tests
are above
tests. The data a depth
from ofthe1.2 µmload
step where the
tests ISE
are is not
also shownveryforsignificant.
comparison. TheThe
plotdata
shows thethe
from strength of the
CLH tests
are above a depth of 1.2 µm where the ISE is not very significant. The plot shows the strength of the
current
are above testing
a depthmethodology
of 1.2 µm where wherein a combination
the ISE of step loadThe
is not very significant. tests
plotand CLHthe
shows tests is usedofto
strength
current testing methodology wherein a combination of step load tests and CLH tests is used to
measure
the currentthe strain
testing rate dependence
methodology of hardness
wherein over seven
a combination orders
of step loadoftests
magnitude
and CLH in the
testsstrain ratetoby
is used
measure the strain rate dependence of hardness over seven orders of magnitude in the strain rate by
a single
measure theinstrument in a simple of
strain rate dependence and quick over
hardness manner. sevenIt orders
is interesting to note
of magnitude thatstrain
in the the strain
rate byrate
a
a single instrument in a simple and quick manner. It is interesting to note that the strain rate
sensitivity,
single instrument which inisa the slope
simple of the
and quickdata, changes
manner. It isaround a strain
interesting rate of
to note 1033the
that 1/s.strain
This will
rate be discussed
sensitivity,
sensitivity, which is the slope of the data, changes around a strain rate of 10 1/s. This will be discussed
in greater
which is the detail
slope ofin the
the data, changes around a strain rate of 103 1/s. This will be discussed in greater
next section.
in greater detail in the next section.
detail in the next section.

Figure
Figure 9. 9. Indentation
Indentation hardness
hardness asas a function
a function ofof strain
strain rate
rate during
during the
the constant
constant load
load and
and hold
hold (CLH)
(CLH)
Figure 9. Indentation hardness as a function of strain rate during the constant load and hold (CLH)
test
test and
and step
step load
load test.
test.
test and step load test.
 Materials 2017, 10, 663 10 of 12
Materials 2017, 10, 663 10 of 12
3.3. Equivalent Uniaxial Response
In this Uniaxial
3.3. Equivalent section, Response
we present the equivalent uniaxial strain rate and stress calculated from the
indentation data, and the comparison with the uniaxial data from the literature. The procedure to
In this section, we present the equivalent uniaxial strain rate and stress calculated from the
calculate the equivalent uniaxial strain rate and stress is described in Section 2.5. Figure 10 shows the
indentation data, and the comparison with the uniaxial data from the literature. The procedure to
equivalent uniaxial stress as a function of equivalent uniaxial strain rate calculated from the
calculate the equivalent uniaxial strain rate and stress is described in Section 2.5. Figure 10 shows the
indentation data and conventional uniaxial testing. Results from uniaxial testing for this alloy over
equivalent uniaxial stress as a function of equivalent uniaxial strain rate calculated from the indentation
the range of strain rates achieved in this work are obtained from Khan et al. [21]. The low strain rate
data and conventional uniaxial testing. Results from uniaxial testing for this alloy over the range of
data is from uniaxial compression testing, while the high strain rate data is from direct disc impact
strain rates achieved in this work are obtained from Khan et al. [21]. The low strain rate data is from
tests. In order to compare the results of this work where a Berkovich tip is used, which induces an
uniaxial compression testing, while the high strain rate data is from direct disc impact tests. In order to
equivalent strain of 8%, uniaxial results at two different strains (5% and 10%) are shown in the plot.
compare the results of this work where a Berkovich tip is used, which induces an equivalent strain of
The indentation data at 8% strain, lies within the region bounded by the uniaxial data at 5% and 10%,
8%, uniaxial results at two different strains (5% and 10%) are shown in the plot. The indentation data
over a wide range of strain rates. Given the vast differences in test geometries and test protocols
at 8% strain, lies within the region bounded by the uniaxial data at 5% and 10%, over a wide range of
between the uniaxial and indentation tests, it is very interesting to note that the indentation data
strain rates. Given the vast differences in test geometries and test protocols between the uniaxial and
matches the uniaxial data over seven orders of magnitude in strain rate. The difference in the uniaxial
indentation tests, it is very interesting to note that the indentation data matches the uniaxial data over
data at two different strain levels indicates that steady state conditions may not have been achieved
seven orders of magnitude in strain rate. The difference in the uniaxial data at two different strain
during indentation which induces 8% equivalent strain. This is similar to the observations of Luthy
levels indicates that steady state conditions may not have been achieved during indentation which
et al. [22] who performed torsion tests to very high strain (300–1000%) in order to achieve steady state
induces 8% equivalent strain. This is similar to the observations of Luthy et al. [22] who performed
creep in pure aluminum at room temperature. While the results of the current work may not
torsion tests to very high strain (300–1000%) in order to achieve steady state creep in pure aluminum
represent steady state conditions, the experimental procedure and analysis presented here provide a
at room temperature. While the results of the current work may not represent steady state conditions,
generic framework to measure strain rate dependence of stress over a wide range of strain rates with
the experimental procedure and analysis presented here provide a generic framework to measure
a high degree of precision.
strain rate dependence of stress over a wide range of strain rates with a high degree of precision.

Figure 10. Comparison of equivalent uniaxial strain rate and stress calculated from the indentation
Figure 10. Comparison of equivalent uniaxial strain rate and stress calculated from the indentation
data with the uniaxial results from conventional compression test and direct disc impact test (Khan
data with the uniaxial results from conventional compression test and direct disc impact test
et al. [21]).
(Khan et al. [21]).

4. Summary and Conclusions

4. Summary and Conclusions
Advances in instrumentation have enabled nanomechanical measurements with very low noise
Advances in instrumentation have enabled nanomechanical measurements with very low noise
levels (sub nanometer) at fast time constants (20 µs) and high data acquisition rates (100 KHz). These
levels (sub nanometer) at fast time constants (20 µs) and high data acquisition rates (100 KHz). These
capabilities in conjunction with a comprehensive model for instrument’s dynamics and electronics is
capabilities in conjunction with a comprehensive model for instrument’s dynamics and electronics is
vital for accurate high strain rate measurements.
vital for accurate high strain rate measurements.
The indentation system used in this work is shown to be extremely well characterized by a
The indentation system used in this work is shown to be extremely well characterized by a simple
simple one DOF harmonic oscillator model which can be readily extended to testing under non-
one DOF harmonic oscillator model which can be readily extended to testing under non-ambient
ambient conditions (vacuum or high temperature).
conditions (vacuum or high temperature).
Materials 2017, 10, 663 11 of 12

A comprehensive model for the instrument’s dynamics and electronics has been presented to
accurately factor out the instrument’s contribution to the measurement during a high strain rate test
and validated with the step load experiments in free air. The importance of having fast measurement
time constants for accurate high strain rate measurements has been demonstrated.
Step load tests have been performed on commercial purity aluminum (1100 Al), wherein the force
is ramped to the desired level as fast as the instrument can physically accomplish the change, thereby
enabling access to a range of high strain rates (>1000 1/s) in a single indentation test.
A simple procedure has been presented to determine the hardness and indentation strain rate
during a step load test. The strain rate dependence of hardness has been measured over seven orders
of magnitude by a combination of step load and CLH tests.
The uniaxial equivalent strain rate and stress calculated from the indentation data closely matches
the uniaxial results over seven orders of magnitude. Given the vast differences in test geometries and
test protocols between the uniaxial and indentation tests, it is very encouraging that the indentation
data matches the uniaxial data over several orders of magnitude in strain rate.
The experimental procedure and analysis presented in this work provides a generic framework
to measure strain rate dependence of stress over a wide range of strain rates with a high degree
of precision in a simple, quick, and cost-effective way compared to the conventional methods.
The simplicity of this experimental technique also enables it to be extended to high temperatures,
thereby facilitating the measurement of a high strain rate response at elevated temperatures, which is
a largely unexplored challenging area of research/experimentation.

Author Contributions: P.S.P. and W.C.O. conceived and designed the experiments; P.S.P. performed the
experiments; P.S.P. and W.C.O. analyzed the data; P.S.P. wrote the paper.
Conflicts of Interest: The authors declare no conflict of interest.

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